JP4590601B2 - Library analyzer - Google Patents

Description

The present invention relates to a library analysis apparatus suitable for analyzing a plurality of, for example, several tens or more samples prepared by mixing a plurality of types of raw materials at different ratios. In particular, the present invention relates to a library analyzer capable of automatically analyzing a plurality of samples forming composition points of a multi-component composition diagram and displaying the analysis results.

Taking inorganic materials as an example, recent advances in fine ceramic technology have made it possible to control the crystal structure, composition, and crystal grain size of ceramic materials on the micron to nanoscale. For this reason, the development of application of ceramic materials to electronic materials and the like is rapidly expanding. Among these, ceramic oxides have a wide range of physical properties in terms of dielectric properties, magnetic properties, electrical conductivity, and the like. The diversity of functions of ceramic materials means that the parameters to be controlled as ceramic materials are extremely diverse, including their non-stoichiometry and crystal structure anisotropy.

As a result, ceramic materials obtained by mixing and firing multiple types of inorganic material raw materials that are starting materials at different ratios as in the conventional method are manufactured one by one, and their properties are examined. Not only does it take an enormous amount of time to reach, it is extremely unlikely to lead to accidental discoveries that are beyond intuition and experience. Furthermore, when handling the same type of substance with a plurality of people, the probability of an error due to human error increases.

In searching for new ceramic materials, it is possible to automatically analyze materials in addition to systematically controlling the combination of various raw materials by using an automatic processor. Become important. In other words, it is possible to effectively search for new ceramic materials by automating the analysis of materials so that an enormous variety of materials are not accumulated without being analyzed.

In the case of organic material raw materials as an example, it is well known that, for example, in the field of pharmaceuticals, combinatorial techniques are also widely adopted in the development of effective drugs. In this field as well, it is possible to analyze a large number of samples with different mixing ratios accurately and in a short time in addition to mixing multiple types of raw materials. The search for new materials in the science and technology field can be expected to make great progress.

The inventors have invented and applied for a patent for a chemical reaction processing apparatus that generates and analyzes a large number of samples obtained by mixing a plurality of inorganic material raw materials in different ratio combinations (Patent Document 1). By using this chemical reaction processing apparatus, a large number of chemical products can be obtained and analyzed and evaluated by easy control.

As a method for analyzing a chemical product, a method using X-rays, infrared rays, or the like is general and effective (Patent Documents 2 and 3). However, analysis of individual characteristics of a large number of chemical products obtained by combinatorial techniques using conventional methods takes a long time and can be one of the major obstacles to material search.

JP 2001-219052 A JP 2000-338061 A JP 2002-202255 A

The present invention makes the above-described chemical reaction apparatus developed by the present inventors more effective. For example, a plurality of kinds of raw materials are mixed by using a combinatorial method and mixed at various ratios. It is an object of the present invention to provide a library analyzer capable of automatically generating a sample and automatically analyzing a library placed on a library plate.

The present invention provides a library analyzer capable of automatically calculating the positions of a plurality of samples at predetermined sample formation points on a library plate and automatically measuring the characteristics of individual samples individually. It is to provide.

That is, the present invention is (1) a library analyzer for analyzing a library in which a plurality of samples are formed at predetermined sample formation points on a library plate, wherein the sample has different ratios of a plurality of types of raw materials. The library analyzer is provided with a library production means, a control means, an input means, and a measurement means, and is input from the input means by the library production means. Based on the chemical treatment conditions, the control means automatically executes each element operation of weighing, mixing, drying, and heat treatment to form a plurality of samples at a plurality of sample formation points on the raw material library plate. manufacture, X-axis to the measuring means, coordinate and X-axis in the Y axis direction, the reference point on the Y axis is defined in advance, with a predetermined position relationship between the reference point And an X-axis and a Y-axis of the positions of the plurality of sample forming points based on data relating to the positions of the plurality of sample forming points on the library plate input from the input means. Deviation from the reference point in the direction is calculated by the control means, and the measurement probe is sequentially moved to the sample formation point based on the deviation calculated by the control means, and each sample at the sample formation point is A library analyzer characterized by being individually measured.

As the measuring means, known measuring means such as X-ray diffraction measurement, infrared spectroscopic measurement, dielectric constant measurement, and electrical conductivity measurement can be employed. For example, X-rays or infrared rays are made into thin beams and each sample is irradiated sequentially, the probe is brought into contact with or in close proximity to the sample, and the dielectric constant and electrical conductivity are measured. A plurality of probes can be arranged, and measurement can be performed while changing the probe to be measured. For example, if the measurement probe is provided at the tip of a flexible optical fiber or electric wire, the measurement probe can be easily moved, and the apparatus can be simplified and effective.

It is also effective to observe the change in the state of a substance by video. Specifically, each sample is photographed with an imaging device such as a CCD camera or an infrared camera, the entire library is photographed, or the position on the library plate is associated with the position of the image to change the state of the sample. Can be measured for each sample formation point as a change in shape or a change in temperature.

If the entire library analyzer is set on the coordinates consisting of the X and Y axes, the position of the reference point and the sample formation point on the library plate can be easily expressed as coordinate points on the coordinates consisting of the X and Y axes. It is possible to easily calculate each positional relationship.

The present invention also provides (2) a library analyzer for analyzing a library in which a plurality of samples are formed at predetermined sample formation points on a library plate, wherein the samples have different ratios of a plurality of types of raw materials. The library analysis apparatus is provided with a library manufacturing means, a control means, an input means, and a measurement means, and is input from the input means by the library manufacturing means. Based on the chemical treatment conditions, the control means automatically executes each element operation of weighing, mixing, drying, and heat treatment, and the combination ratio of the plurality of raw materials is set to the plurality of sample formation points on the library plate. as the ratio of the composition point of composition diagram of dimensions corresponding to the number of kinds of raw material, to produce a library with a plurality of samples, X-axis to the measuring means, A coordinate point in the axial direction and reference points on the X and Y axes are determined in advance, and provided with a library plate support that is movable in the X and Y axis directions and moves the sample formation point to the measurement point. Deviations from the reference points in the X-axis and Y-axis directions of the sample formation points are calculated by the control means based on data relating to the positions of a plurality of sample formation points on the library plate input from the input means. The library is characterized in that, based on the deviation calculated by the control means, the support table is automatically transferred so that the sample formation point sequentially moves to the measurement point, and the measurement is sequentially performed. Analyzer.

Although the reference point can be set at an arbitrary position, it is preferable to set the measurement point as the reference point because the calculation for moving the sample formation point to the measurement point becomes easy. The X direction and the Y direction indicate two axes that form a plane, and express the moving surface of the support base. Although there is no particular limitation, when the sample is powder, it is preferable to form a horizontal plane in order to stably hold the sample.

The present invention also provides a library analyzer above SL (2), that the combination ratio of a plurality of raw material of the sample have been made and the ratio of the composition point of composition diagram of dimensions corresponding to the number of kinds of the raw material A library analyzer characterized by this.

The composition diagram is a three-dimensional composition diagram when there are three kinds of raw materials and is called a ternary composition diagram. Moreover, when there are four types of raw materials, a quaternary composition diagram is obtained. The number of coordinate divisions is the number when the side connecting the vertices is divided into several at equal intervals, and the number of lines when the lines are drawn at equal intervals parallel to each side. The intersecting point or the point on the side is the composition point, and indicates the composition ratio.

Further, the present invention provides: (3) In the library analyzer of the above (2 ), the support base rotates around the measurement point, and the data input from the input means to the control means A library analyzer, wherein the support is automatically rotated after the sample formation point is automatically moved to the measurement point.

By automatically rotating the support table, even an anisotropic sample can be measured independent of the measurement direction.

According to the present invention, (4) in the library analyzer of the above (1), (2) or (3 ) , the library analyzer is provided with an analysis means, and the plurality of samples have different codes. The characteristics of the plurality of samples measured are stored in the analysis means as a file for each code, the library analyzer is connected to a database of substances, and the characteristics stored for each code A library analyzer, wherein the characteristics of the sample and the characteristics of each substance in the database are automatically collated by the analysis means.

As the database, for example, a publicly known one such as a JCPDS file which is an X-ray diffraction data file or a database constructed independently can be used. Further, a known method such as peak search can be employed as a method for collation. The code is not particularly limited, but it is preferable to use numbers and alphabets because identification is easy. In particular, it is preferable to employ numbers because the numbers indicate where the sample is located in the composition diagram. It is preferable that the code is given in advance according to the type of the library and stored in the control means because the configuration can be simplified.

Moreover, a pure compound can be found easily by collating with the characteristic of a database. Here, the pure compound is a compound obtained when one kind of chemical product is obtained from the mixed raw materials, and means a sample having no impurities. If the conditions under which a pure compound can be obtained are understood, the target material can be obtained efficiently and with high purity.

In addition, the present invention provides: (5) In the library analyzer of the above (4) , the library analyzer includes display means capable of displaying a composition diagram, and the analysis result can be displayed on the composition diagram. A library analyzer characterized by having

According to the library analyzer of the present invention, a huge number of samples on the library plate can be automatically analyzed. In addition, if the sample is mixed at a ratio that changes the raw materials regularly, the characteristics of the sample having a finer composition ratio than the composition ratio of the sample to be analyzed can be estimated from the continuity of the characteristic change. For example, an accurate pure substance can be searched using a composition diagram. That is, since the degree of coincidence of characteristics with the pure substance can be evaluated for each composition point, it is possible to search for a pure compound at a position deviating from the composition point according to the number of divisions.

Hereinafter, embodiments of the present invention will be described with reference to the drawings. FIG. 1 is a block diagram showing an embodiment of the library analyzer of the present invention, FIG. 2 is a plan view showing the main part of the measuring means of the library analyzer of the present invention, and FIG. FIG. 4 is a cross-sectional view showing the main part of the measuring means of another library analyzer, FIG. 4 is a composition diagram of the division number of coordinates 10 displayed on the display means of the library analyzer of the present invention, and FIG. FIG. 6 is a composition diagram corresponding to the division number 10 displaying the analysis result by the library analyzer of the present invention, and FIG. 6 is a flowchart showing the analysis method by the library analyzer of the present invention.

(Embodiment 1)
A case where a liquid inorganic material raw material is used as a raw material and a chemical product (sample) is analyzed by X-ray diffraction will be described as an example. In FIG. 1, the control means 1 is connected to the input means 2, the display means 3, the analysis means 4, the database 5, the measurement means 6, the library manufacturing means 7, and the transport means 8 through electrical communication means.

As shown in FIG. 2, the library manufacturing means 7 manufactures a library in which a plurality of samples 9 are formed at a plurality of predetermined sample forming points 63 on the library plate 62. The sample 9 is a chemical product obtained by mixing a plurality of kinds of raw materials in a combination of different ratios, and the ratio is a ratio of composition points in a composition diagram of a dimension corresponding to the number of types of raw materials. The library manufactured by the library manufacturing means 7 is transferred to the measuring means 6 by the transport means 8 and is installed on the library support 61.

Since the number of samples made by mixing multiple raw materials in different ratio combinations becomes enormous, it is possible to reduce the enormous amount of work by automatically manufacturing the library, and human error It is also possible to avoid. Further, if the library plate 62 is automatically transferred, it is possible to automate from library manufacture to library analysis, so that the work process can be reduced and the effect of avoiding human error is increased.

Next, a method for automatically manufacturing a library will be described. In the input means 2, (1) identification names and concentrations of plural types of raw materials to be mixed, (2) the number of divisions of coordinates in the composition diagram, and (3) chemical processing conditions of the raw materials to be mixed are input as data. The method for inputting the identification name is performed by inputting the raw material name, inputting the concentration in the identification name previously shown on the input screen provided in the input means, or selecting the identification name. The raw material name and the identification name are made to correspond separately.

The chemical treatment condition is a condition of each element operation for library manufacture.
The amount of the sample to be formed on 2 and when performing the reaction by heating, are drying and heating conditions. When automatically performing from library manufacture to library analysis, (4) library analysis conditions are input from the input means 2 in addition to the chemical processing conditions.

These data inputted from the input means 2 are sent to the control means 1. In the control means 1,
A composition diagram having dimensions corresponding to the number of types of raw materials input from the input means 2 is created. next,
Different signs are given to the composition points determined by the number of divisions input from the input means 2.
Here, the composition point is determined by equally dividing the ratio of each raw material contained in a mixture obtained by mixing a plurality of types of raw materials by the number of divisions. Mixing ratios of a plurality of raw materials at the composition points corresponding to these codes are automatically calculated, and samples 9 having different mixing ratios are automatically generated by the library manufacturing means 7.

Further, the control unit 1 automatically executes each element operation relating to chemical processing such as placing the sample 9 on the sample formation point 63 on the library plate 62, drying, and heating. The arrangement is performed by automatically arranging a plurality of samples 9 on the library plate 62 by a predetermined amount according to the chemical processing conditions input by the input means 2. Further, the plurality of samples 9 on the library plate 62 are automatically dried and heated according to the chemical processing conditions input by the input means 2. In this way, the library is manufactured.

The library obtained as described above is automatically and sequentially measured with predetermined X-rays by the measuring means 6 in accordance with the analysis conditions input from the input means 2. Subsequently, the analysis unit 4 automatically analyzes the measurement result obtained by the measurement unit 6. As described above, the plurality of samples 9 are assigned different codes, and the measured characteristics of the plurality of samples 9 are stored in the analyzing unit 4 as files for each code. Further, the characteristics of the sample 9 stored for each code and the characteristics of the known substance stored in the database 5 are automatically verified by the analysis means 4.

The measuring means 6 includes a support 61 for the library plate 62 shown in FIG.
A coordinate axis in the X-axis and Y-axis directions and a reference point 64 on the X-axis and Y-axis are determined in advance. The library plate 62 is fixed to a recess in which the library plate 62 provided on the support base 61 is fitted. The support base 61 is movable in the X-axis and Y-axis directions.
In other words, the sample formation points 63, 63,...
It is made to move by a transfer device (not shown).

That is, a plurality of sample formation points 63 on the library plate 62 input from the input means 2
, 63,... Are calculated by the control means 1 in the X-axis and Y-axis directions from the reference point 64 of the measuring means 6 to the sample forming points 63, 63,. Based on the deviation calculated by the control means 1, the support base 61 is moved so that the sample formation points 63, 63,... Automatically move sequentially to the measurement points.

When the sample has anisotropy, the measurement is performed while the support base 61 is automatically rotated around the measurement point set at the position of the reference point 64. In this way, non-directional X-ray diffraction can be measured. If anisotropy is expected in the sample, the control means 1 automatically performs these operations if the input means 2 inputs that there is anisotropy as an analysis condition.

The center of the library plate 62 when the support 61 is placed at the start position before the measurement is the reference point 64, and the coordinate points on the X axis and Y axis of the reference point 64 are stored in the control means 1. Yes. Based on the information of the library plate 62 input from the input means 2, deviations on the X-axis and Y-axis of the 66 sample forming points 63, 63, 63,. The Further, information on the deviation of the sample formation point 63 from the reference point 64 is recorded in advance in the control means 1 for each type of the library plate 62, and collated with the type of the library plate 62 inputted from the input means 2. Thus, the deviation may be obtained.

The upper left corner 65 of the library plate 62 is cut off, and the corner portion bulges to fit in the corresponding position of the support base 61. Therefore, the library plate 62 is installed in the wrong direction. There is nothing. That is, there is no mistake in the order of the samples.

The display means 3 displays a composition diagram corresponding to the number of coordinate divisions. In addition, the analysis result obtained by the analysis means 4 is displayed on the composition diagram.

The library analyzer according to the present invention will be described more specifically. Each unit in FIG. 1 is unitized, and a library analyzer can be configured by combining various units. That is, as a combination of the library analyzers, the control unit 1, the input unit 2, and the measurement unit 6 are the minimum combination, and can be combined as a control unit, an input unit, and a measurement unit, respectively.

Here, the measuring means 6 is an X-ray measuring unit. Display means 3, if necessary
The analysis means 4 and the database 5 can be provided as a display unit, an analysis unit, and a database unit. It is also effective to add the library manufacturing means 7 and the transport means 8 as a library manufacturing unit and a transport unit in order to automatically perform from library manufacture to library analysis. Further, the database 5 is a control means 1 through a communication line.
By connecting with, you can also use an external database.

As the control means 1, a personal computer is used. The input means 2 employs a keyboard and a mouse. The display means 3 is composed of a liquid crystal screen. The input means 2 is preferably a touch panel system using the display means 3 because the operation is simple. The control means 1 weighs, mixes, arranges, dries, heat-treats each raw material according to the identification name of a plurality of kinds of raw materials input from the input means 2, corresponding to the proportion of each composition point equally. -It has a function to automatically and continuously execute each element operation such as X-ray diffraction and analysis. Further, the control unit 1 is connected to analysis means 4 that performs collation analysis. The analysis unit 4 has a function of performing phase identification by collating with the database 5 and displaying the analysis result shown on the composition diagram on the display unit 3.

Here, if a pure compound is identified at a certain composition point, and the same compound as the pure compound and another compound are identified at an adjacent composition point, the pure compound is also identified between one composition point and the next composition point. There is a high possibility. For example, when it can be determined that the proportion of other compounds is small, it can be determined that there is a high possibility that a pure compound is identified even near the adjacent composition point, and a composition diagram with a larger number of divisions can be obtained. Based on this, a sample in the vicinity of the adjacent composition point is manufactured, and the identification of the pure compound is repeated in the same manner, whereby the range in which the pure compound is obtained can be accurately determined.

In the library manufacturing means 7, a liquid inorganic material raw material was weighed and dispensed with a dispensing pipette, and the sample in the dispensed mixing container was mixed using a stirring bar to produce a sample. Samples are collected and arranged with a preparative pipette, arranged on a platinum library plate 62 having a sample forming portion 63 having 66 recesses (wells), dried and heated to produce a library. Heating is performed by firing the placed sample in an electric furnace.

The measuring means 6 measures X-ray diffraction lines of the sample 9 constituting the library, and converts the recorded data into a format that can be collated with an X-ray diffraction data file (for example, JCPDS file) stored in the database 5. It is a line measurement unit. Further, the data has a function of outputting for each code of the sample in a one-to-one correspondence with each sample 9 on the library plate 62.

The analysis unit 4 stores each data output from the measurement unit 6 sent via the control unit 1 in the analysis unit as a file for each code, and stores the X-ray data file (for example, JCPDS file) stored in the database 5. ), The operation of extracting the known phase in the product and extracting the diffractogram of the unknown phase is performed. The analysis means 4 extracts diffraction patterns for all the samples on the library plate 62, and when the number of starting materials is n, the analysis verification result is plotted in the n-dimensional space and displayed on the composition diagram. A composition diagram plotting this product can be registered. Here, it is preferable that the combination of the types of raw materials, the chemical treatment conditions, and the analysis conditions can be stored as data because the number of operations can be reduced.

(Embodiment 2)
A case where an inorganic fine powder is used as a raw material and a chemical product (sample) is analyzed for vitrification state using visible light will be described as an example. The library is manufactured by weighing and mixing a plurality of kinds of inorganic fine powders, placing them on the library plate 62, and heating them. As shown in FIG. 3, a sample 9 which is a chemical product obtained by mixing a plurality of kinds of raw materials in combinations of different ratios at predetermined sample formation points 63, 63,. Is formed. The ratio of the plural types of raw materials of the sample 9 is a ratio that changes regularly in an arithmetic series. For example, the ratio of each raw material contained in the sample 9 is expressed in mol%, and is changed at a constant ratio such as every 10%. Further, the surface of the sample formation point 63 of the library plate 62 is all colored black.

Next, the measuring means 6 will be described. The measuring means 6 has coordinate axes in the X-axis and Y-axis directions, a reference point 64 on the X-axis and Y-axis, and a support base 61 are fixed, and can be moved in the X-axis and Y-axis directions and the sample. A measurement probe 66 capable of measuring 64 characteristics is provided.
A plurality of sample formation points 63, 63,... On the library plate 62 inputted from the input means 2
... Based on the data relating to the positions of the measuring means 6, deviations in the X-axis and Y-axis directions of the positions of the plurality of sample forming points 63, 63,. The Based on the deviation calculated by the control means 1, the measurement probe 66 is sequentially moved to the sample formation points 63, 63,.

A black and white camera is used as the probe 66, and if the sample is vitrified, the transparency is good, so the black is photographed, and the degree of vitrification can be known from the density of the photographed sample. it can. As the lang = EN-US> probe, a monochrome camera that captures the entire library plate 62 is used instead of a monochrome camera that individually captures the sample, and the position on the library plate 62 and the position of the image are associated with each other. The vitrification state of the sample can also be measured for each sample formation point as the shade of the image.

Next, an embodiment of library analysis using the library analyzer of the present invention will be described. As an example of the synthesis of a specific substance, an analysis of a ternary ramsdellite type crystal phase expected as a positive electrode material for a lithium secondary battery will be given and described with reference to FIG.

As a liquid inorganic material raw material which is a starting material, (1) chromium acetate (Cr (OCOCH ₃ ) ₃
) 0.5 mol / l aqueous solution, (2) Lithium hydroxide hydrate (LiOH.H ₂ O) 1.
0 mol / l aqueous solution and (3) titanium oxide (TiO ₂ ) slurry concentration with water as dispersion medium 1
. Three types of 0 mol / l were used.

First, in the input step 11, the identification names of the above three kinds of liquid inorganic material raw materials, their molar concentrations, the number of divisions of the coordinates of the composition diagram, and the chemical treatment conditions and the analysis conditions from the input means 2 to the control means 1
Entered in. At this time, the liquid inorganic material raw material was selected by entering the concentration in the raw material 1, raw material 2, and raw material 3 displayed on the screen as the identification names. When the input is completed, the composition diagram creation step 12 is executed, and the composition diagram 31 shown in FIG. In this case, the combination of the composition ratios of the raw materials is 66.

Further, in the range setting step 13, the range of the composition diagram displayed on the display unit 3 by the input unit 2 is set. Here, the entire range of the composition diagram was set. The setting of the range is set only for generating a sample to be analyzed in the composition diagram. In this way, unnecessary operations can be excluded, and the efficiency of research can be increased. Subsequently, a mixing ratio calculation step 14 was executed, and 66 kinds of mixing ratios of the three kinds of inorganic material raw materials were automatically calculated according to the set total range of the composition diagram and the division number 10 of the coordinates of the composition diagram.

Subsequently, in the sample generation step 15, 66 samples having different mixing ratios were automatically generated according to the chemical processing conditions. Here, the chemical treatment conditions refer to the stirring time, stirring conditions, and the like of the liquid inorganic material raw material and, if necessary, the conditions such as the atmospheric temperature and the atmospheric gas.

Subsequently, in the arranging step 16, the 66 liquid samples are automatically arranged on the one platinum library plate 62 having the sample forming parts 63 which are 66 recesses (wells) according to the chemical processing conditions. did. Here, the chemical treatment conditions are the serving amount, tray temperature, ambient temperature,
It refers to drying conditions for atmospheric gases and liquid samples.

In the heat treatment step 17, a plurality of samples on the library plate were automatically heat-treated according to the chemical treatment conditions. Here, the chemical treatment conditions include a temperature rising rate, a heating temperature, a heating time, a cooling rate, an atmospheric gas, and the like. As shown in FIG. 5, the heating temperature is an absolute temperature of 11
Heating was performed at 73 degrees, 1273 degrees, and 1373 degrees for a predetermined time. That is, three samples in which the sample 9 was placed on the library plate 62 were manufactured, and three types of libraries were manufactured under different heating conditions. The atmosphere gas was air.

The library plate 62 on which the library is manufactured is a support base 6 of the measuring means 6 by manual operation.
1 was fixed on top. Subsequently, in the measurement step 18, the support base 61 was automatically transferred so that the sample formation point 63 automatically moved to the measurement point. Further, for each of the 66 samples heat-treated on the library plate 62, the support base 61 automatically rotates while X
The line diffraction lines were measured, and the recorded data was converted into a format that can be collated with an X-ray diffraction data file (JCPDS file) stored in the database 5. Data was output for each sample code in a one-to-one correspondence with each sample 9 on the library plate 62.

The analysis conditions in this step include the X-ray irradiation angle, X-ray intensity, rotation of the support table, and the like. Further, since measurement of X-ray diffraction lines required 5 minutes per sample, measurement of 66 samples required 5 hours 30 minutes. However, since all of the 66 samples were automatically measured, it was possible to use the night without human intervention.

Further, in the analysis step 19, the X-ray diffraction line measurement result was automatically analyzed according to the analysis conditions. That is, each data output from the measuring means 6 sent via the control means 1 is collated with an X-ray data file (JCPDS file) stored in the database 5, and a ramsdellite crystal which is a known phase in the product. Extracted. Here, since diffraction patterns are extracted for all samples on the library plate 62 and the number of raw materials is 3, the analysis verification result is plotted in a three-dimensional space and displayed on the composition diagram as shown in FIG. did. Here, the analysis conditions refer to the type of database to be collated, analysis conditions, and the like.

The analysis result in the analysis step 19 was written on the original composition diagram for each temperature as shown in FIG. The composition 34 in which the ramsdellite crystal phase was observed is indicated by a black circle. These were pure compounds. On the composition diagram at an absolute temperature of 1373 degrees, the ramsdellite crystal phase was observed in the widest range. Further, in order to specify the range in which the ramsdellite crystal phase can be obtained in detail, it is possible to increase the number of divisions in the range 33 of the composition diagram shown in FIG. 5 and manufacture the sample.

Although the embodiments of the present invention have been described with reference to the drawings, the specific configuration of the present invention is not limited to these embodiments, and the present invention can be changed even if there is a design change or the like without departing from the gist of the present invention. include. For example, the composition diagram is not limited to a three-component system and may be a four-component system or more. For example, in a four-component system, a composition diagram can be visually displayed with a triangular pyramid. The number of coordinate divisions may be less than 10 or more than 20. Of course, the number may be between 10 and 20. The range may be set by enclosing the range with a surrounding line, or may be set by selecting a combination of compositions one by one. The library plate is not limited to a substrate, but may be a crucible or other test container mounted on a holding device.

According to the library analyzer of the present invention, even a composition in which a plurality of inorganic material raw materials are mixed at a mixing ratio of several tens to several hundreds can be efficiently and accurately analyzed. Can handle numbers and facilitates discovery of new substances. The same effect can be obtained when a plurality of organic material raw materials are targeted.

It is a block diagram which shows the Example of the library analyzer of this invention. It is a top view which shows the principal part of the measurement means of the library analyzer of this invention. It is sectional drawing which shows the principal part of the measurement means of the other library analyzer of this invention. It is a composition diagram of the division | segmentation number 10 of the coordinate displayed on the display means of the library analyzer of this invention. It is a composition figure corresponding to the number of divisions 10 which displayed the analysis result by the library analyzer of the present invention. It is a flowchart which shows the analysis method by the library analyzer of this invention.

Explanation of symbols

DESCRIPTION OF SYMBOLS 1 Control means 2 Input means 6 Measuring means

Claims (5)

A library analyzer for analyzing a library in which a plurality of samples are formed at predetermined sample formation points on a library plate,
The sample is a chemical product obtained by mixing a plurality of types of raw materials in different ratio combinations,
The library analyzer includes a library manufacturing means, a control means, an input means, and a measuring means,
Based on the chemical processing conditions input from the input unit, the library manufacturing unit automatically executes each element operation of weighing, mixing, drying, and heating processing by the control unit, so that a plurality of raw material on the library plate A library is manufactured by forming multiple samples at the sample formation point of
The measuring means includes coordinate axes in the X-axis and Y-axis directions and reference points on the X-axis and Y-axis, and includes a library plate support having a predetermined positional relationship with the reference points. ,
Deviations from the reference points in the X-axis and Y-axis directions of the positions of the plurality of sample forming points based on the data relating to the positions of the plurality of sample forming points on the library plate input from the input means are controlled. Calculated by means,
The measurement probe is sequentially moved to the sample formation point based on the deviation calculated by the control means, and each sample at the sample formation point is individually measured. Library analyzer. A library analyzer for analyzing a library in which a plurality of samples are formed at predetermined sample formation points on a library plate,
The sample is a chemical product obtained by mixing a plurality of types of raw materials in different ratio combinations,
The library analyzer includes a library manufacturing means, a control means, an input means, and a measuring means,
A plurality of samples on the library plate are automatically executed by the control means on the basis of the chemical processing conditions input from the input means by the library manufacturing means, and the weighing means, mixing, drying, and heat treatment are performed by the control means. A library is produced by forming a plurality of samples such that the combination ratio of the plurality of raw materials is a ratio of composition points of a composition diagram of a dimension corresponding to the number of types of the raw materials at the formation point,
The measurement means has coordinate axes in the X-axis and Y-axis directions, and reference points on the X-axis and Y-axis, and is a library plate that is movable in the X-axis and Y-axis directions and moves the sample formation point to the measurement point. Is equipped with a support base,
Deviations from the reference points in the X-axis and Y-axis directions of the sample formation points are calculated by the control means based on data relating to the positions of a plurality of sample formation points on the library plate input from the input means. ,
The library analysis is characterized in that, based on the deviation calculated by the control means, the support base is automatically transferred so that the sample formation point sequentially moves to the measurement point, and the measurement is sequentially performed. apparatus. The support is rotated around the measurement point. After the sample formation point is automatically moved to the measurement point according to the data input from the input means, the support is automatically that is adapted to rotate in claim 2 Symbol placement of the library analyzer characterized. The library analyzer is provided with analysis means,
The plurality of samples are given different signs from each other,
The measured characteristics of the plurality of samples are stored in the analysis means as a file for each code,
The library analyzer is connected to a substance database, and the characteristics of the sample stored for each code and the characteristics of each substance in the database are automatically collated by the analyzing means. The library analyzer according to claim 1, 2 or 3 . The library analyzer includes a display unit capable of displaying composition diagram, claim 4 Symbol mounting of the library analyzer characterized in that it is adapted to be able to display the analysis result on the composition diagram.

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